Hippolyte eugene serullas



(No Model.)

H. E. SRULLAS. PROCESS 0F BXTRAGTING AND PURIPYING GUTTA PERGHJL No. 544,934.

Patented Aug. 20, 18954.

FIE

Pula

W/ TNE SSE S.'

A TTUHNE Y J' u NITFD STATES `ATENT OFFICE- HIPPOLYTE EUGENE sERULLAs, oF FORT DE LEAU, ALGERIA.

PROCESS OF EXTRACTING AND PURIFYING GUTTA-PERCHA.

SPECIFICATION formingpart of Letters Patent N o. 544,934, dated August 20, 1895.

To a/ZZ whom t may concern:

rBe it known that I, HIPPOLYTE EUGENE SERULLAS, a citizen of the Republic of France, residing in Fortde lEau, Algeria, have invented an Improvement in the Process for the Extraction and Purification of GuttalFercha, of which the following is a specifica- 1on.

My invention has for its object the extraction of gutta-percha from the young shoots or buds and other like parts and,preferably, from the leaves of the isonandra, while preserving absolutely intact the electrical properties of vthis product--that is to say, obtaining it in a Condition suitable for covering the cores of submarine cables. During scientific expeditions in the Malay Archipelago I have learned the proportions of this gum existing in the different parts of the plants of the sapota or sapodilla family and the possibility of substituting very advantageously, in place of the present primitive and wasteful man-` ner of.obtaining the gutta-percha, a rational and economical use of the stalks, buds, leaves, and other parts of the isonandra without having to sacrifice the trunk of the trees.

There are obviously only two processes for obtaining the gatta-percha 'from the leaves and other parts of the isonandra. Either to directly dissolve out only this gum, leaving insoluble all the other substances, or to eliminate these substances successively, leaving the pure gutta as the final residue. The former of these processes destroys the structure of the laticiferous cells. The three hydrocarbons-namely, gatta, fluavil, and alban-forming the constituent parts of these cells in the soncmdras 19e/reha (Hooker) have each very notable differences of solubility. It results that when they are separated from the solvents they are precipitated in some manner in distinct lots, according tothe order of their respective solubility. It then becomes exceedingly difficult, if not impossible, to accurately re-establish their original composition by mixing, grinding, or by any other mechanical means. There is still another objection to this former process. These parts are no longer inclosed in the special cells in which they were found before being dis- Application filed March 16 1893.

Serial No. 466,247. (No model.)

solved. In place `of an aggregation of cells there now only exists a mixture, more or less homogeneous, of a hydrocarbon and two resins. The gum, besides being deprived of all its tenacity before Working it up, in which .process the Malay natives submit it in warm water, instead of taking a fibrous texture under the rollers after its extraction by the aid of the solvents, in consequence of a considerablel elongation of` the adhering `or consolidated cells, becomes a simple depressed magma ot' rather a horny appearance, losing erous cells, enables the product to retain.

these last-named properties, which are indis pensable in the manufacture of cables. This latter process is that to which my invention relates.

Preliminary operations-The material under treatment is rst dried in a stove in an atmosphere of carbonic-acid gas at a temperature not exceeding 63 centigrade; secondly, pulverized; thirdly, water is drained or washed through at the temperature of the drying process, in order to avoid the coagulation of certain albuminoid matters which an alkaline solution would not remove.

First operation (chemt'caZ).-When the washing water from the vegetable powder flows away colorless I pour the powder, along with the water of the last washing, into a digester or closed vessel provided with a valve which will only allow an internal pressure of about eight atmospheres. Icover this saturated powder Wit-h about twenty centimeters of water, to which is added potash or soda in the proportion of three parts, by weight, of the alkali to one hundred parts of the powder being treated, or a carbonate of one of these alkalies may be employed containing the base in the same proportion. I keep the contents of the digester at a temperature varying between 106 and 108 centigrade for two hours. Care must be taken that the temperature does notreach 110 centigrade, at which tempera- IOO ture thefiuavil would begin to be injured anddecomposed. I then pour the contents both liquid and solid onto a filter, where the residue should be thoroughly washed. I preferably effect this washing by the process known as filtration by section, and with watts raised to ak temperature of about 8Oo centigrade. The washing lis completed when the water comes out of the. filter clear and without color and without any action on red litmus-paper.

Second operation (che1m`caZ).-Tlie residue or settlement thus washed is then poured into an enameled pan, adding sufficient water to cover it with liquid of about ve or six centimeters in depth. This water has preferably added to it hydrochloric acid in the proportion of one and a half parts for every hundred parts of the initial weight of the powder, which in the preceding operation has been reduced to nearly threefourths of its original weight. The pan in which the treatment with acidulated water takes place is provided with a mechanical agitator and a false or double bottom, permitting of heating by steam. When the mixture has been heated for about half an hour at a temperature near the boiling point of water under a pressure of seven hundred and sixty millimeters, I pour out the contents of the pan into a filter, washing it several times on the said filter with warm water, as inthe preceding operation. The wash# ing is completed when the water ceases to turn blue litmus-paper red.

Third operation (mecham'caZ).-The residue thus obtained is compressed, then spread out under a press at a temperature slightly above o centigrade. I then wash it for a little while in running water not exceeding 50 centigrade Ain temperature. The solid mass thus gets rid of a portion of the interposed cellular or cellulosic powder.

Fourth operation (mccha'm'caZ).-The impure gutta-percha, which forms the solid residue after the mechanical treatment above described, is then triturated in a pug-mill, then passed under rollers, where it is spread out in very thin sheets.

The pugmill and rollers which I employ may be analogous to those usually employed for the purification of ordinary gutta-percha of commerce.

Fifth operation (chemicaZ).-'l`hese sheets of gutta-percha thus produced are then stretched on metallic frames which may be arranged to fit in the grooves of a wooden chest lined with metal (zinc or galvanized sheet iron). I introduce these frames into the grooves, which are vertical, so arranged that the space between any two consecutive sheets is from five to six millimeters. I then pass slowly through the said chest a streaml of ammonia having in solution precipitated oxide of copper-in other words, a stream of which, as seen through a magnifying-, g;lass`,

appear to be full of small holes, are placed in a drying pug-mill similar to those usually en1- ployed in the manufacture of gutta-perche.. They are there hardened and agglutinated, after which it only remains to roll them afresh or, better still, to compress them into cakes for better preservation.-

In order to enable the treatment described under fifth heading to be better understood and what is essential, I will now briefiy describe the apparatus which is indispensable for obtaining the complete elimination of the cellulose, and that without injuring in any degree the properties of the gutta-percha.

In the accompanying drawings, Figure l is a View showing the different vessels in section in their different positions. Fig. 2 is a sectional plan of the chest A. y

A is the chest or washer, which contains the metal frames over which are stretched the sheets of gutta-percha. The ammoniacal copper liquor enters by the pipe a and leaves by the pipe b. A

t is a glass-gage tube with metal socket and funnel.

B is the still, heated by steam or water bath, Whose goose-necked pipe c brings back in solution in the water recovered ammoniacal gas. Cl is the reservoir containing the ammoniacal water; D, a small barrel or cylinder having an internal agitator or rouser of any known kind (paddles, for example) and in which the solution of the oxide of copper is effected. v

E is the receiver for the copper ammoniacal liquor, whence it flows into the chest A.

'm are safety-tubes, and r cocks for working the apparatus.

One chest A is preferably fed by several sets of apparatus B, C, D, and E.

I claim as my inventionl. A process of extracting gutta percha consisting in treating the parts of the tree with an alkali or its carbonate,"then treating this residue with dilute hydrochloric acid, at the same time triturating it, then spreading this last residue into sheets and then treating the sheets to a stream of ammoniacal copper liquid, substantially as set forth.

2. Aprocess of extracting gutta percha con- IOC IIC

sisting in treating the parts of the tree with an alkali or its carbonates then treating the name to this specification in the residue with dilute sulphuric acid, next spreading this last residue out into sheets and treating thesheets first with a stream of am moniacal copper liquid and afterward with a current of carbonio gas or hydrogen gas,

substantially as set forth.

In testimony whereof I have signed my presence of ro two subscribing witnesses.

HIPPOLYTE EUGNE -SRULLAS Witnesses:

FELIX HOURAND, CHARLES THEODORE GRELLET. 

